CN114908340B - Ultrathin copper foil with carrier and preparation method thereof - Google Patents
Ultrathin copper foil with carrier and preparation method thereof Download PDFInfo
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- CN114908340B CN114908340B CN202210627115.8A CN202210627115A CN114908340B CN 114908340 B CN114908340 B CN 114908340B CN 202210627115 A CN202210627115 A CN 202210627115A CN 114908340 B CN114908340 B CN 114908340B
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000011889 copper foil Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011888 foil Substances 0.000 claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 43
- 239000000956 alloy Substances 0.000 claims abstract description 43
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 238000000151 deposition Methods 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 27
- 230000001699 photocatalysis Effects 0.000 claims abstract description 22
- 239000011941 photocatalyst Substances 0.000 claims abstract description 22
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 20
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 20
- 229910017709 Ni Co Inorganic materials 0.000 claims abstract description 17
- 229910003267 Ni-Co Inorganic materials 0.000 claims abstract description 17
- 229910003262 Ni‐Co Inorganic materials 0.000 claims abstract description 17
- 239000003792 electrolyte Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 11
- 238000009713 electroplating Methods 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 10
- 238000004070 electrodeposition Methods 0.000 claims description 9
- 239000004519 grease Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 102000008186 Collagen Human genes 0.000 claims description 6
- 108010035532 Collagen Proteins 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 6
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 6
- 229940044175 cobalt sulfate Drugs 0.000 claims description 6
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 6
- 229920001436 collagen Polymers 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- 150000002085 enols Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000007747 plating Methods 0.000 description 22
- 230000008021 deposition Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005137 deposition process Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1657—Electroless forming, i.e. substrate removed or destroyed at the end of the process
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1664—Process features with additional means during the plating process
- C23C18/1667—Radiant energy, e.g. laser
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
- C25D5/44—Aluminium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
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Abstract
The invention discloses an ultrathin copper foil with a carrier, which comprises a metal foil carrier layer, an alloy layer and an ultrathin copper foil layer; the thickness of the ultrathin copper foil layer is 1-4 mu m, and the ultrathin copper foil layer is deposited on the alloy layer by a photocatalytic deposition method; the alloy layer is deposited on the metal foil carrier layer by electroplating, and the electrolyte is Ni-Co alloy solution containing rare earth element Ce. The invention also provides a preparation method of the ultra-thin copper foil with the carrier, which comprises the following steps: (1) pre-treating the metal foil carrier layer; (2) electrodepositing an alloy layer on the surface of the metal foil carrier layer; (3) depositing an ultrathin copper foil layer on the surface of the alloy layer: an ultra-thin copper foil layer is formed on the metal foil carrier layer by a photocatalytic deposition method in a copper sulfate mixed solution containing a photocatalyst. The invention can obtain the ultrathin copper foil which can be stably separated from the carrier, and the stripped ultrathin copper foil has good compactness and uniformity, excellent tensile property and capability of improving the ultrathin copper foil performance while reducing the thickness of the copper foil.
Description
Technical Field
The invention relates to the technical field of preparation of ultrathin copper foil with a carrier, in particular to an ultrathin copper foil with a carrier and a preparation method thereof.
Background
In recent years, with the high integration and miniaturization of electronic products such as mobile phones, computers, and digital cameras, a printed wiring board (Printed Circuit Board, abbreviated as PCB) and a lithium battery for electronic products are required to be lighter, thinner, and lighter. The electrolytic copper foil is a base material of a negative electrode current collector of a PCB and a lithium ion battery, and under such a trend, development and research of the electrolytic copper foil tend to be thinner and have higher performance. The smaller the thickness of the copper foil, the less easy the long-distance transportation and long-term storage, and the more easy the crease and tear occur in the use process. The ultrathin copper foil is electrodeposited on a carrier to prepare the ultrathin copper foil with the carrier, and the ultrathin copper foil with the carrier is supported by the carrier, so that the problem that the ultrathin copper foil is difficult to transport and store can be well solved.
The thickness of the ultrathin copper foil produced by the current domestic manufacturer is mainly 6-9 mu m, the process difficulty of the existing electrolytic copper foil process for preparing the ultrathin copper foil below 6 mu m is high, the further lightening and thinning of the copper foil are important directions of the current copper foil industry development aiming at the requirements of lighter, thinner, cost reduction and synergy, the thickness of the ultrathin copper foil is reduced, and simultaneously, the larger performance breakthrough is realized, so that the requirement of diversified production is met, and the important and difficult problems of the development of the ultrathin copper foil are realized.
Disclosure of Invention
The present invention aims to solve the above technical problems existing in the prior art. The ultra-thin copper foil with the carrier and the preparation method thereof provided by the invention can be used for obtaining the ultra-thin copper foil which can be stably separated from the carrier, and the stripped ultra-thin copper foil has good compactness and uniformity, excellent tensile property and capability of improving the ultra-thin copper foil while reducing the thickness of the copper foil.
In order to solve the technical problems, the embodiment of the invention discloses an ultrathin copper foil with a carrier, which comprises a metal foil carrier layer, an alloy layer and an ultrathin copper foil layer;
the thickness of the ultrathin copper foil layer is 1-4 mu m, and the ultrathin copper foil layer is deposited on the alloy layer by a photocatalytic deposition method;
the alloy layer is deposited on the metal foil carrier layer through electroplating, and the electrolyte is Ni-Co alloy solution containing rare earth element Ce.
Further, an ultraviolet lamp with the power of 140-160W is adopted in the photocatalytic deposition method, the characteristic wavelength is 254.6nm, the distance between the ultraviolet lamp and the quartz reactor is 50mm, and the ultraviolet lamp irradiates for 0.2-1h.
Further, the metal foil carrier layer is 35 μm aluminum foil.
Further, the peel strength between the ultra-thin copper foil layer and the metal foil carrier layer is 0.14-0.20N/mm.
The embodiment of the invention also discloses a preparation method of the ultra-thin copper foil with the carrier, which comprises the following steps:
(1) Pretreating the metal foil carrier layer to remove grease and an oxide layer on the surface of the metal foil carrier layer;
(2) Electrodepositing an alloy layer on the surface of the metal foil carrier layer: the electrolyte used for electrodeposition is Ni-Co alloy solution containing rare earth element Ce;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer: an ultra-thin copper foil layer having a thickness of 1-4 μm is formed on the metal foil carrier layer by a photocatalytic deposition method in a copper sulfate mixed solution containing a photocatalyst.
Further, in the step (2), the electrodeposition conditions are: the electrolyte temperature is 45 ℃, the pH is 4, and the current density is 15-20A/dm 2 。
Further, in the Ni-Co alloy solution containing the rare earth element Ce in the step (2), 10-25g/L of nickel sulfate, 20-50g/L of cobalt sulfate, 0.1-0.5g/L of cerium sulfate, 20g/L of boric acid, 5-10g/L of sodium chloride and 0.5-2.5g/L of sodium dodecyl sulfate are added.
Further, in the step (3), the composition of the copper sulfate mixed solution is as follows: 90g/L copper sulfate, 100g/L sulfuric acid, 30ppm hydrolyzed collagen, 40ppm hydrochloric acid, 2-5g/L glyceryl tristearate and a photocatalyst.
Further, in the step (3), the photocatalyst is prepared by the following method: dropwise adding one of 5g/L tetrabutyl titanate, 7g/L enol silyl ether and 5g/L dibutyl tin dilaurate into 15-30g/L absolute ethyl alcohol under stirring, adding ultrapure water after the dropwise adding is finished, continuously stirring for 1-3h, placing the obtained mixed solution into a baking oven at 60-75 ℃, drying, grinding a sample obtained after the drying, and finally calcining at 400-550 ℃ for 0.5-1.5h to obtain the photocatalyst.
Further, in step (1), the grease is removed by washing with an acetone solution;
the oxide layer was removed by using a mixed aqueous solution of nitric acid (65-68 wt% concentration level), 5% sulfuric acid (98 wt% concentration level) and 5% hydrofluoric acid (40 wt% concentration level) at a volume concentration of 50%.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the invention, 35 mu m aluminum foil is used as a carrier, after the surface of the aluminum foil is pretreated, a Ni-Co alloy stripping layer containing rare earth elements Ce is deposited on the surface of the aluminum foil, and finally, a carrier-attached ultrathin copper foil layer is prepared by a photocatalytic deposition method;
the rare earth element Ce is introduced into the Ni-Co alloy, so that the stability of the plating solution can be improved, the cathode polarization of the plating solution is increased, the precipitation of hydrogen at a cathode is reduced, the grains of the plating layer are refined, the corrosion resistance of the plating layer is improved, the stripping resistance of the plating layer is improved, and the plating performance is improved; in addition, when the rare earth element Ce is compounded with the alloy layer, the excellent stripping effect can be realized only by a small addition amount;
the thickness of the ultrathin copper foil can be strictly controlled by a photocatalytic deposition method, the obtained ultrathin copper foil can be stably separated from a carrier, and the stripped ultrathin copper foil has good compactness and uniformity, excellent tensile property and can improve the performance of the ultrathin copper foil while reducing the thickness of the copper foil;
the preparation method provided by the invention is simple and easy to operate.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present specification, by describing the embodiments of the present invention with specific examples. While the description of the invention will be described in connection with the preferred embodiments, it is not intended to limit the inventive features to the implementation. Rather, the purpose of the invention described in connection with the embodiments is to cover other alternatives or modifications, which may be extended by the claims based on the invention. The following description contains many specific details for the purpose of providing a thorough understanding of the present invention. The invention may be practiced without these specific details. Furthermore, some specific details are omitted from the description in order to avoid obscuring the invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
Example 1
(1) Pretreatment of a metal foil carrier layer
Taking 35 mu m aluminum foil as a carrier, cleaning the surface of the aluminum foil by using an acetone solution, removing impurities such as surface grease and the like, and removing an oxide layer on the surface of the aluminum foil by using a mixed aqueous solution of nitric acid, sulfuric acid and hydrofluoric acid;
(2) Depositing an alloy layer on the surface of a metal foil carrier layer
The aluminum foil in the step (1) is used as a carrier layer, the alloy layer is deposited in Ni-Co plating solution, the Ni-Co plating solution contains 20g/L of nickel sulfate, 30g/L of cobalt sulfate, 0.1g/L of cerium sulfate, 20g/L of boric acid, 6g/L of sodium chloride, 0.6g/L of sodium dodecyl sulfate, the plating solution temperature is 45 ℃, the PH value is 4, and the current density is 15A/dm 2 The electrodeposition time is 8s;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer
Placing the aluminum foil subjected to the alloy plating in the step (2) into a copper sulfate mixed solution containing a photocatalyst for photocatalytic deposition to obtain an ultrathin copper foil with the thickness of 4 mu m;
composition of copper sulfate electrolyte: 90g/L copper sulfate, 100g/L sulfuric acid, 30ppm hydrolyzed collagen, 40ppm hydrochloric acid, 2g/L glyceryl tristearate and a photocatalyst;
preparing a photocatalyst: dropwise adding 5g/L tetrabutyl titanate into 25g/L absolute ethyl alcohol under stirring, adding ultrapure water after the dropwise adding is completed, continuously stirring for 1h, placing the obtained mixed solution into a 60 ℃ oven for drying, grinding a sample obtained after the drying, and finally calcining for 1.5h at 400 ℃ to obtain a photocatalyst;
technological parameters of photocatalytic deposition: an ultraviolet lamp with the power of 150W and the characteristic wavelength of 254.6nm, wherein the distance between the ultraviolet lamp and the quartz reactor is 50mm, and the ultraviolet lamp irradiates for 0.5h.
Example 2
(1) Pretreatment of a metal foil carrier layer
Taking 35 mu m aluminum foil as a carrier layer, cleaning the surface of the aluminum foil by using an acetone solution, removing impurities such as surface grease and the like, and removing an oxide layer on the surface of the aluminum foil by using a mixed aqueous solution of nitric acid, sulfuric acid and hydrofluoric acid;
(2) Depositing an alloy layer on a metal foil carrier surface
The aluminum foil in the step (1) is used as a carrier layer, the alloy layer is deposited in Ni-Co plating solution, the Ni-Co plating solution contains 25g/L of nickel sulfate, 27g/L of cobalt sulfate, 0.5g/L of cerium sulfate, 20g/L of boric acid, 5g/L of sodium chloride, 1g/L of sodium dodecyl sulfate, the plating solution temperature is 45 ℃, the PH value is 4, and the current density is 18A/dm 2 The electrodeposition time is 10s;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer
Placing the aluminum foil subjected to the alloy plating in the step (2) into a copper sulfate mixed solution containing a photocatalyst for photocatalytic deposition to obtain an ultrathin copper foil with the thickness of 3 mu m;
composition of copper sulfate electrolyte: 90g/L copper sulfate, 100g/L sulfuric acid, 30ppm hydrolyzed collagen, 40ppm hydrochloric acid, 5g/L glyceryl tristearate and a photocatalyst;
preparing a photocatalyst: dropwise adding 7g/L enol silyl ether into 30g/L absolute ethyl alcohol under stirring, adding ultrapure water after dropwise adding, continuously stirring for 1.5 hours, placing the obtained mixed solution into a 66 ℃ oven for drying, grinding a sample obtained after drying, and finally calcining for 1 hour at 435 ℃ to obtain the photocatalyst;
photocatalytic deposition process parameters: an ultraviolet lamp with the power of 150W and the characteristic wavelength of 254.6nm, wherein the distance between the ultraviolet lamp and the quartz reactor is 50mm, and the ultraviolet lamp irradiates for 0.5h.
Example 3
(1) Pretreatment of a metal foil carrier layer
Taking 35 mu m aluminum foil as a carrier, cleaning the surface of the aluminum foil by using an acetone solution, removing impurities such as surface grease and the like, and removing an oxide layer on the surface of the aluminum foil by using a mixed aqueous solution of nitric acid, sulfuric acid and hydrofluoric acid;
(2) Depositing an alloy layer on a metal foil carrier surface
Taking the aluminum foil in the step (1) as a carrier, and alloying in a Ni-Co plating solutionThe deposition of the layer, ni-Co plating solution contains 18g/L of nickel sulfate, 35g/L of cobalt sulfate, 0.2g/L of cerium sulfate, 20g/L of boric acid, 8g/L of sodium chloride, 2g/L of sodium dodecyl sulfate, the plating solution temperature is 45 ℃, the PH value is 4, and the current density is 20A/dm 2 The electrodeposition time is 10s;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer
Placing the aluminum foil subjected to the alloy plating in the step (2) into a copper sulfate mixed solution containing a photocatalyst for photocatalytic deposition to obtain an ultrathin copper foil with the thickness of 3.5 mu m;
composition of copper sulfate electrolyte: 90g/L copper sulfate, 100g/L sulfuric acid, 30ppm hydrolyzed collagen, 40ppm hydrochloric acid, 3g/L glyceryl tristearate and a photocatalyst;
preparing a photocatalyst: dropwise adding 5g/L dibutyl tin dilaurate into 15g/L absolute ethyl alcohol under stirring, adding ultrapure water after the dropwise adding is completed, continuously stirring for 2 hours, placing the obtained mixed solution into a 75 ℃ oven for drying, grinding a sample obtained after the drying, and finally calcining at 550 ℃ for 0.5 hour to obtain the photocatalyst;
photocatalytic deposition process parameters: an ultraviolet lamp with the power of 150W and the characteristic wavelength of 254.6nm, wherein the distance between the ultraviolet lamp and the quartz reactor is 50mm, and the ultraviolet lamp irradiates for 0.5h.
Example 4
An ultra-thin copper foil layer having a thickness of 3 μm was obtained in the same manner as in example 2, except that the photocatalytic deposition process parameters in step (3) were replaced with an ultraviolet lamp having a success rate of 140W, and the ultraviolet lamp was irradiated for 1 hour.
Example 5
An ultra-thin copper foil layer having a thickness of 2.5 μm was obtained in the same manner as in example 2, except that the photocatalytic deposition process parameters in step (3) were replaced with an ultraviolet lamp having a success rate of 150W, and the ultraviolet lamp was irradiated for 0.2 hours.
Example 6
An ultra-thin copper foil layer having a thickness of 1 μm was obtained in the same manner as in example 2, except that the photocatalytic deposition process parameters in step (3) were replaced with an ultraviolet lamp having a success rate of 160W, and the ultraviolet lamp was irradiated for 0.2 hours.
Comparative example 1
(1) Pretreatment of a metal foil carrier layer
Taking 35 mu m aluminum foil as a carrier, cleaning the surface of the aluminum foil by using an acetone solution, removing impurities such as surface grease and the like, and removing an oxide layer on the surface of the aluminum foil by using a mixed aqueous solution of nitric acid, sulfuric acid and hydrofluoric acid;
(2) Depositing an alloy layer on a metal foil carrier surface
The aluminum foil in the step (1) is used as a carrier layer, the alloy layer is deposited in Ni-Co plating solution, the Ni-Co plating solution contains 25g/L of nickel sulfate, 27g/L of cobalt sulfate, 0.5g/L of cerium sulfate, 20g/L of boric acid, 5g/L of sodium chloride, 1g/L of sodium dodecyl sulfate, the plating solution temperature is 45 ℃, the PH value is 4, and the current density is 18A/dm 2 The electrodeposition time is 10s;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer
Placing the aluminum foil subjected to the alloy plating in the step (2) into copper sulfate electrolyte for copper electroplating to obtain an ultrathin copper foil with the thickness of 6 mu m;
composition of copper sulfate electrolyte: 90g/L copper sulfate, 100g/L sulfuric acid, 30ppm hydrolyzed collagen and 40ppm hydrochloric acid; the current density was 30A/dm 2 The temperature of the electrolyte is 55 ℃, and the deposition time is 35s;
comparative example 2
An ultrathin copper foil layer having a thickness of 4 μm was obtained in the same manner as in comparative example 1, except that the electrolytic process parameters in step (3) were replaced with a current density of 20A/dm 2 The deposition time was 20s.
Comparative example 3
An ultra-thin copper foil layer having a thickness of 3 μm was obtained in the same manner as in comparative example 1, except that the electrolytic process parameters in step (3) were replaced with a current density of 20A/dm 2 The deposition time was 15s.
Performance testing
Samples prepared in examples 1-6 and comparative examples 1-3 were laminated with FR-4 prepreg at 180℃and tested for peel strength by mechanical means on carrier foils. Further, performance test was performed on the ultra-thin copper foil after peeling, and the results are shown in table 1.
TABLE 1
Test results show that the ultra-thin copper foil layers and the aluminum foil carrier in the embodiments 1-6 have excellent stripping effect, the stripping strength is 0.14-0.20N/mm, and the surface of the ultra-thin copper foil after stripping is bright and clean and has no tearing and wrinkling. The peel strength of the sample of the example is smaller than that of the sample of the comparative example, because the photocatalytic deposition method utilizes the photocatalytic copper salt to directly deposit copper on the surface of the aluminum foil, the obtained ultrathin copper foil has good compactness and uniformity and is easier to be completely peeled from the carrier. In addition, the example samples had a thinner thickness and higher tensile strength than the control samples.
While the invention has been described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing is a further detailed description of the invention in connection with specific embodiments, and it is not intended to limit the invention to the specific embodiments described. Various changes in form and detail may be made therein by those skilled in the art, including a few simple inferences or alternatives, without departing from the spirit and scope of the present invention.
Claims (5)
1. The carrier-attached ultrathin copper foil is characterized by comprising a metal foil carrier layer, an alloy layer and an ultrathin copper foil layer;
the thickness of the ultrathin copper foil layer is 1-4 mu m, the ultrathin copper foil layer is deposited on the alloy layer by a photocatalytic deposition method, an ultraviolet lamp with the power of 140-160W is adopted in the photocatalytic deposition method, the characteristic wavelength is 254.6nm, the ultraviolet lamp is 50mm away from a quartz reactor, and the ultraviolet lamp irradiates for 0.2-0.5h;
the alloy layer is deposited on the metal foil carrier layer through electroplating, and the electrolyte is Ni-Co alloy solution containing rare earth element Ce;
the preparation method of the ultra-thin copper foil with the carrier comprises the following steps:
(1) Pretreating the metal foil carrier layer to remove grease and an oxide layer on the surface of the metal foil carrier layer;
(2) Electrodepositing an alloy layer on the surface of the metal foil carrier layer: the electrolyte used for electrodeposition is Ni-Co alloy solution containing rare earth element Ce;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer: forming an ultrathin copper foil layer with the thickness of 1-4 mu m on the metal foil carrier layer by a photocatalytic deposition method in a copper sulfate mixed solution containing a photocatalyst;
in the step (3), the composition of the copper sulfate mixed solution is as follows: 90g/L copper sulfate, 100g/L sulfuric acid, 30ppm hydrolyzed collagen, 40ppm hydrochloric acid, 2-5g/L glyceryl tristearate and a photocatalyst;
the photocatalyst is prepared by the following method: dropwise adding one of 5g/L tetrabutyl titanate, 7g/L enol silyl ether and 5g/L dibutyl tin dilaurate into 15-30g/L absolute ethyl alcohol under stirring, adding ultrapure water after the dropwise adding is finished, continuously stirring for 1-3h, placing the obtained mixed solution into a baking oven at 60-75 ℃, drying, grinding a sample obtained after the drying, and finally calcining at 400-550 ℃ for 0.5-1.5h to obtain the photocatalyst;
in the step (2), the electrodeposition conditions are: the electrolyte temperature is 45 ℃, the pH is 4, and the current density is 15-20A/dm 2 ；
In the Ni-Co alloy solution containing rare earth element Ce, nickel sulfate 10-25g/L, cobalt sulfate 20-50g/L, cerium sulfate 0.1-0.5g/L, boric acid 20g/L, sodium chloride 5-10g/L and sodium dodecyl sulfate 0.5-2.5g/L.
2. The ultra-thin copper foil with carrier according to claim 1, wherein the metal foil carrier layer is 35 μm aluminum foil.
3. The ultra-thin copper foil with carrier according to claim 1, wherein the peel strength between the ultra-thin copper foil layer and the metal foil carrier layer is 0.14 to 0.20N/mm.
4. A method for preparing the ultra-thin copper foil with carrier according to any one of claims 1 to 3, comprising the steps of:
(1) Pretreating the metal foil carrier layer to remove grease and an oxide layer on the surface of the metal foil carrier layer;
(2) Electrodepositing an alloy layer on the surface of the metal foil carrier layer: the electrolyte used for electrodeposition is Ni-Co alloy solution containing rare earth element Ce;
(3) Depositing an ultrathin copper foil layer on the surface of the alloy layer: an ultra-thin copper foil layer having a thickness of 1-4 μm is formed on the metal foil carrier layer by a photocatalytic deposition method in a copper sulfate mixed solution containing a photocatalyst.
5. The method for producing an ultra-thin copper foil with carrier according to claim 4, wherein in the step (1), the grease is removed by washing with an acetone solution;
the oxide layer is removed by using a mixed aqueous solution of 65-68wt% strength grade nitric acid, 5% 98wt% strength grade sulfuric acid, and 5% 40wt% strength grade hydrofluoric acid at a volume concentration of 50%.
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